Korean Journal of Food Science and Technology (한국식품과학회지)

Korean Society of Food Science and Technology (한국식품과학회)
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A Survey of Zearalenone in Beans Using High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FLD) and Ultra Performance Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)

HPLC-FLD 및 LC-MS/MS에 의한 두류 중 제랄레논 오염실태 조사

  • 장미란 (부산지방식품의약품안전청 시험분석센터) ;
  • 이창희 (부산지방식품의약품안전청 시험분석센터) ;
  • 이효정 (부산지방식품의약품안전청 시험분석센터) ;
  • 김지연 (부산지방식품의약품안전청 시험분석센터) ;
  • 손상혁 (부산지방식품의약품안전청 시험분석센터) ;
  • 신춘식 (부산지방식품의약품안전청 시험분석센터) ;
  • 김소희 (부산지방식품의약품안전청 시험분석센터) ;
  • 김대병 (부산지방식품의약품안전청 시험분석센터)
  • Published : 2008.06.30
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Abstract

A survey for zearalenone contamination was conducted on 27 soy bean samples, 27 red bean samples, 16 black bean samples, 19 seoritae samples, 14 seomoktae samples, for a total of 127 commercial Korean samples. Zearalenone was quantified by the immunoaffinity column clean-up method with high performance liquid chromatography-fluorescence detection (HPLC-FLD), and was confirmed by liquid chromatography tandem mass spectrometry(LC-MS/MS). The limits of detection and quantification were $2.0{\mu}g/kg$ and $6.0{\mu}g/kg$, respectively. The recovery in the beans ranged from 82.2 to 98.4%. According to HPLC-FLD, zearalenone was detected in 13 samples (10.2% incidence), including 1 soybean and 12 red bean samples. The zearalenone contamination levels were in the range of 8.01${\sim}38.98{\mu}g/kg$. Finally, LC-MS/MS analysis was conducted in the contaminated samples to verify the results of HPLC-FLD. The LC-MS/MS results confirmed the presence of zearalenone in all 13 samples. The contamination level was lower than that of EU, which is below $100{\mu}g/kg$ for raw grains.

국내유통 중인 대두, 붉은콩, 검은콩 녹두 등 6품목의 두류 총 127건을 immunoaffinity column 정제방법 및 HPLC-FLD을 이용하여 제랄레논에 대한 오염실태를 조사하였다. 상관계수($R^2$) 0.999 이상으로 양호한 직선성을 보였고 검출한계 및 정량한계는 각각 2.0 ${\mu}g/kg$, 6.0 ${\mu}g/kg$, 회수율 82.2-98.4%로 나타났다. RSD가 0.82-6.40%로 양호한 재현성을 나타내었다. 모니터링 결과, 대두(백태) 27건 중 1건(3.7%)에서 37.62 ${\mu}g/kg$ 검출되었고 붉은콩(팥) 27건 중 12건 검출되어 44.4%의 검출율을 보였고 그 오염수준은 8.01-38.98 ${\mu}g/kg$이었다. 나머지 시료 검정콩 16건, 녹두 24건, 서리태(속청) 19건, 서목태(약콩) 14건에서는 모두 검출되지 않았다. 따라서 총 시료 127건 중 13건 검출되어 10.2%의 검출율을 보였고 그 오염수준은 8.01-38.98 ${\mu}g/kg$이었다, 검출시료 13건을 LCMS/MS로 확인한 결과 모두 제랄레논임이 확인되었다. 본 연구결과에서 나타난 두류의 검출빈도 및 오염수준은 유럽연합에서 설정된 기준규격 이하의 수준이었으나 곰팡이독소의 생성의 특이성을 고려한다면 지속적이고 광범위하게 오염실태 조사가 되어야 한다고 판단된다.

Keywords

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